data_bodieite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'bodieite' _chemical_compound_source 'Tintic district, Utah' _chemical_formula_sum 'Bi2 O10 S Te2' _chemical_formula_weight 865.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Bi' 'Bi' -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'I 2/a' _space_group_name_Hall '-I 2ya' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 8.1033(8) _cell_length_b 7.4302(8) _cell_length_c 14.6955(17) _cell_angle_alpha 90 _cell_angle_beta 97.771(9) _cell_angle_gamma 90 _cell_volume 876.68(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 6.555 _exptl_crystal_F_000 1464 _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.005 _exptl_crystal_size_min 0.005 _exptl_absorpt_coefficient_mu 46.894 _shelx_estimated_absorpt_T_min 0.256 _shelx_estimated_absorpt_T_max 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 7132 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.078 _diffrn_reflns_theta_max 25.017 _diffrn_reflns_theta_full 25.017 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 769 _reflns_number_gt 665 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+1.3197P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_extinction_coef 0.00015(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 769 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0347 _refine_ls_wR_factor_gt 0.0330 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Bi Bi 0.03575(4) 0.14587(5) 0.18313(2) 0.01273(12) Uani 1 1 d . . . . . Te Te 0.14779(7) 0.57599(7) 0.11271(3) 0.01133(16) Uani 1 1 d . . . . . S S 0.250000 0.1053(4) 0.000000 0.0133(7) Uani 1 2 d S T P . . O1 O 0.1056(8) 0.2185(9) 0.0109(4) 0.0324(17) Uani 1 1 d . . . . . O2 O 0.2816(8) 0.9948(8) 0.0836(4) 0.0257(16) Uani 1 1 d . . . . . O3 O 0.9258(7) 0.2384(8) 0.3051(3) 0.0167(14) Uani 1 1 d . . . . . O4 O 0.8773(7) 0.3690(7) 0.1228(3) 0.0143(13) Uani 1 1 d . . . . . O5 O 0.1942(7) 0.3890(7) 0.2008(3) 0.0130(13) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi 0.01199(19) 0.0112(2) 0.01584(19) -0.00079(14) 0.00482(13) -0.00070(15) Te 0.0107(3) 0.0122(3) 0.0114(3) 0.0010(2) 0.0028(2) 0.0005(2) S 0.0129(17) 0.0148(18) 0.0130(15) 0.000 0.0049(13) 0.000 O1 0.037(4) 0.042(4) 0.018(4) 0.003(3) 0.004(3) 0.024(4) O2 0.029(4) 0.031(4) 0.018(3) 0.018(3) 0.005(3) 0.005(3) O3 0.020(4) 0.018(4) 0.013(3) -0.002(3) 0.006(3) -0.003(3) O4 0.010(3) 0.012(3) 0.022(3) 0.007(3) 0.007(3) 0.006(3) O5 0.011(3) 0.016(4) 0.010(3) 0.005(2) -0.005(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi O4 2.208(5) 1_455 ? Bi O5 2.211(5) . ? Bi O3 2.217(5) 1_455 ? Bi O2 2.580(6) 6_565 ? Bi O5 2.599(5) 7 ? Bi O1 2.722(6) . ? Bi O2 2.856(6) 1_545 ? Bi O3 3.046(6) 4_545 ? Te O3 1.861(5) 4 ? Te O4 1.890(5) 6_565 ? Te O5 1.902(5) . ? Te O4 2.698(5) 1_455 ? Te O1 2.973(6) 5_565 ? Te O1 3.045(7) . ? Te O2 3.342(6) . ? Te O4 3.464(5) 5_665 ? S O1 1.467(6) . ? S O1 1.467(6) 2 ? S O2 1.471(6) 2_545 ? S O2 1.471(6) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Bi O5 74.4(2) 1_455 . ? O4 Bi O3 79.40(19) 1_455 1_455 ? O5 Bi O3 86.7(2) . 1_455 ? O4 Bi O2 72.6(2) 1_455 6_565 ? O5 Bi O2 143.5(2) . 6_565 ? O3 Bi O2 101.93(19) 1_455 6_565 ? O4 Bi O5 136.94(18) 1_455 7 ? O5 Bi O5 65.2(2) . 7 ? O3 Bi O5 83.99(19) 1_455 7 ? O2 Bi O5 150.25(18) 6_565 7 ? O4 Bi O1 70.15(18) 1_455 . ? O5 Bi O1 75.9(2) . . ? O3 Bi O1 148.0(2) 1_455 . ? O2 Bi O1 78.67(19) 6_565 . ? O5 Bi O1 111.56(18) 7 . ? O4 Bi O2 119.84(17) 1_455 1_545 ? O5 Bi O2 87.0(2) . 1_545 ? O3 Bi O2 157.04(18) 1_455 1_545 ? O2 Bi O2 96.27(14) 6_565 1_545 ? O5 Bi O2 73.32(17) 7 1_545 ? O1 Bi O2 49.79(17) . 1_545 ? O4 Bi O3 144.94(18) 1_455 4_545 ? O5 Bi O3 138.76(17) . 4_545 ? O3 Bi O3 108.17(15) 1_455 4_545 ? O2 Bi O3 72.38(18) 6_565 4_545 ? O5 Bi O3 78.05(16) 7 4_545 ? O1 Bi O3 102.55(16) . 4_545 ? O2 Bi O3 64.23(15) 1_545 4_545 ? O3 Te O4 101.9(2) 4 6_565 ? O3 Te O5 94.8(2) 4 . ? O4 Te O5 90.1(2) 6_565 . ? O3 Te O4 90.0(2) 4 1_455 ? O4 Te O4 156.48(15) 6_565 1_455 ? O5 Te O4 68.5(2) . 1_455 ? O3 Te O1 78.93(19) 4 5_565 ? O4 Te O1 121.9(2) 6_565 5_565 ? O5 Te O1 148.0(2) . 5_565 ? O4 Te O1 80.05(17) 1_455 5_565 ? O3 Te O1 149.3(2) 4 . ? O4 Te O1 105.7(2) 6_565 . ? O5 Te O1 72.32(19) . . ? O4 Te O1 59.46(17) 1_455 . ? O1 Te O1 97.20(16) 5_565 . ? O3 Te O2 67.48(19) 4 . ? O4 Te O2 58.40(19) 6_565 . ? O5 Te O2 136.85(19) . . ? O4 Te O2 144.87(16) 1_455 . ? O1 Te O2 69.68(18) 5_565 . ? O1 Te O2 140.01(15) . . ? O3 Te O4 126.23(18) 4 5_665 ? O4 Te O4 88.69(19) 6_565 5_665 ? O5 Te O4 138.26(18) . 5_665 ? O4 Te O4 100.60(12) 1_455 5_665 ? O1 Te O4 52.16(14) 5_565 5_665 ? O1 Te O4 67.93(14) . 5_665 ? O2 Te O4 74.84(13) . 5_665 ? O1 S O1 110.1(6) . 2 ? O1 S O2 111.1(3) . 2_545 ? O1 S O2 106.3(3) 2 2_545 ? O1 S O2 106.3(3) . 1_545 ? O1 S O2 111.1(3) 2 1_545 ? O2 S O2 112.1(5) 2_545 1_545 ? O1 S Bi 122.3(2) . 2 ? O1 S Bi 50.5(2) 2 2 ? O2 S Bi 55.9(2) 2_545 2 ? O2 S Bi 131.2(2) 1_545 2 ? O1 S Bi 50.5(2) . . ? O1 S Bi 122.3(2) 2 . ? O2 S Bi 131.2(2) 2_545 . ? O2 S Bi 55.9(2) 1_545 . ? Bi S Bi 169.86(10) 2 . ? O1 S Bi 86.6(3) . 5 ? O1 S Bi 128.6(2) 2 5 ? O2 S Bi 27.5(2) 2_545 5 ? O2 S Bi 109.8(3) 1_545 5 ? Bi S Bi 79.08(2) 2 5 ? Bi S Bi 106.04(3) . 5 ? O1 S Bi 128.6(2) . 6_655 ? O1 S Bi 86.6(3) 2 6_655 ? O2 S Bi 109.8(3) 2_545 6_655 ? O2 S Bi 27.5(2) 1_545 6_655 ? Bi S Bi 106.04(3) 2 6_655 ? Bi S Bi 79.08(2) . 6_655 ? Bi S Bi 121.08(8) 5 6_655 ? O1 S Te 75.9(3) . 2 ? O1 S Te 40.7(3) 2 2 ? O2 S Te 99.5(3) 2_545 2 ? O2 S Te 144.2(3) 1_545 2 ? Bi S Te 55.95(3) 2 2 ? Bi S Te 113.93(7) . 2 ? Bi S Te 106.07(3) 5 2 ? Bi S Te 125.62(3) 6_655 2 ? O1 S Te 40.7(3) . . ? O1 S Te 75.9(3) 2 . ? O2 S Te 144.2(3) 2_545 . ? O2 S Te 99.5(3) 1_545 . ? Bi S Te 113.93(7) 2 . ? Bi S Te 55.95(3) . . ? Bi S Te 125.62(3) 5 . ? Bi S Te 106.06(3) 6_655 . ? Te S Te 58.28(4) 2 . ? O1 S Te 102.5(3) . 6_665 ? O1 S Te 29.6(2) 2 6_665 ? O2 S Te 133.5(2) 2_545 6_665 ? O2 S Te 87.0(3) 1_545 6_665 ? Bi S Te 79.28(3) 2 6_665 ? Bi S Te 94.90(4) . 6_665 ? Bi S Te 158.15(2) 5 6_665 ? Bi S Te 68.400(13) 6_655 6_665 ? Te S Te 58.33(4) 2 6_665 ? Te S Te 62.00(4) . 6_665 ? O1 S Te 29.6(2) . 5_565 ? O1 S Te 102.5(3) 2 5_565 ? O2 S Te 87.0(3) 2_545 5_565 ? O2 S Te 133.5(2) 1_545 5_565 ? Bi S Te 94.90(4) 2 5_565 ? Bi S Te 79.28(3) . 5_565 ? Bi S Te 68.400(13) 5 5_565 ? Bi S Te 158.15(2) 6_655 5_565 ? Te S Te 62.00(4) 2 5_565 ? Te S Te 58.33(4) . 5_565 ? Te S Te 110.59(7) 6_665 5_565 ? S O1 Bi 104.9(3) . . ? S O1 Te 136.3(3) . 5_565 ? Bi O1 Te 117.2(2) . 5_565 ? S O1 Te 121.0(4) . . ? Bi O1 Te 74.91(14) . . ? Te O1 Te 82.80(16) 5_565 . ? S O1 Te 82.7(3) . 2 ? Bi O1 Te 138.5(2) . 2 ? Te O1 Te 73.85(13) 5_565 2 ? Te O1 Te 66.78(13) . 2 ? S O1 Bi 71.9(2) . 5 ? Bi O1 Bi 117.1(2) . 5 ? Te O1 Bi 78.69(13) 5_565 5 ? Te O1 Bi 161.14(19) . 5 ? Te O1 Bi 104.14(12) 2 5 ? S O2 Bi 137.3(3) 1_565 6_665 ? S O2 Bi 98.8(3) 1_565 1_565 ? Bi O2 Bi 115.3(2) 6_665 1_565 ? S O2 Te 127.1(3) 1_565 . ? Bi O2 Te 78.36(15) 6_665 . ? Bi O2 Te 92.27(15) 1_565 . ? Te O3 Bi 121.5(3) 4_545 1_655 ? Te O3 Bi 130.3(2) 4_545 4 ? Bi O3 Bi 107.76(19) 1_655 4 ? Te O3 Te 122.1(2) 4_545 6_665 ? Bi O3 Te 76.32(13) 1_655 6_665 ? Bi O3 Te 73.46(11) 4 6_665 ? Te O3 Bi 73.65(16) 4_545 7 ? Bi O3 Bi 127.06(19) 1_655 7 ? Bi O3 Bi 82.45(12) 4 7 ? Te O3 Bi 56.59(8) 6_665 7 ? Te O4 Bi 134.9(3) 6_665 1_655 ? Te O4 Te 132.1(2) 6_665 1_655 ? Bi O4 Te 90.99(18) 1_655 1_655 ? Te O4 Te 88.39(18) 6_665 5_665 ? Bi O4 Te 116.23(18) 1_655 5_665 ? Te O4 Te 79.40(12) 1_655 5_665 ? Te O4 Bi 91.40(18) 6_665 4 ? Bi O4 Bi 94.12(17) 1_655 4 ? Te O4 Bi 68.61(12) 1_655 4 ? Te O4 Bi 136.14(16) 5_665 4 ? Te O5 Bi 117.3(2) . . ? Te O5 Bi 126.2(2) . 7 ? Bi O5 Bi 114.8(2) . 7 ? Te O5 Bi 81.71(18) . 4_455 ? Bi O5 Bi 100.01(18) . 4_455 ? Bi O5 Bi 101.71(16) 7 4_455 ? Te O5 Te 80.82(16) . 6_665 ? Bi O5 Te 123.38(19) . 6_665 ? Bi O5 Te 59.89(11) 7 6_665 ? Bi O5 Te 136.52(15) 4_455 6_665 ? _refine_diff_density_max 1.171 _refine_diff_density_min -1.409 _refine_diff_density_rms 0.289 _shelx_res_file ; TITL North Star 3 nostar.res created by SHELXL-2016/6 at 14:28:08 on 23-Dec-2017 CELL 0.71075 8.10333 7.43016 14.69550 90.000 97.771 90.000 ZERR 4 0.00084 0.00075 0.00169 0.000 0.009 0.000 LATT 2 SYMM .50-X, +Y, -Z SFAC BI TE O S UNIT 8 8 40 4 SHEL 99999.000000 0.84000 CONN 8 3.0 Te CONN 8 3.0 Bi OMIT -2 9 3 OMIT 4 3 15 OMIT 2 0 18 OMIT 4 2 16 OMIT 4 0 16 OMIT -1 3 2 OMIT -2 0 6 OMIT 3 7 6 OMIT 5 1 12 OMIT 2 3 15 L.S. 5 FMAP 2 PLAN 8 TEMP 20.0 ACTA SIZE 0.040 0.005 0.005 WGHT 0.000000 1.319700 EXTI 0.000155 FVAR 0.21139 BI 1 0.035750 0.145865 0.183130 11.00000 0.01199 0.01118 = 0.01584 -0.00079 0.00482 -0.00070 TE 2 0.147792 0.575989 0.112712 11.00000 0.01073 0.01223 = 0.01141 0.00102 0.00281 0.00055 S 4 0.250000 0.105338 0.000000 10.50000 0.01285 0.01482 = 0.01304 0.00000 0.00492 0.00000 O1 3 0.105578 0.218526 0.010877 11.00000 0.03709 0.04185 = 0.01821 0.00274 0.00385 0.02400 O2 3 0.281575 0.994812 0.083612 11.00000 0.02873 0.03093 = 0.01810 0.01782 0.00527 0.00541 O3 3 0.925773 0.238445 0.305124 11.00000 0.02040 0.01806 = 0.01278 -0.00173 0.00637 -0.00313 O4 3 0.877263 0.369013 0.122809 11.00000 0.01024 0.01231 = 0.02192 0.00724 0.00737 0.00635 O5 3 0.194228 0.389017 0.200850 11.00000 0.01103 0.01587 = 0.01027 0.00470 -0.00523 -0.00353 HKLF 4 REM North Star 3 REM R1 = 0.0212 for 665 Fo > 4sig(Fo) and 0.0275 for all 769 data REM 70 parameters refined using 0 restraints END WGHT 0.0000 1.3061 REM Highest difference peak 1.171, deepest hole -1.409, 1-sigma level 0.289 Q1 1 0.0264 -0.0356 0.1882 11.00000 0.05 1.17 Q2 1 0.8704 0.3284 0.1744 11.00000 0.05 1.08 Q3 1 0.9774 0.1565 0.3621 11.00000 0.05 0.97 Q4 1 0.2182 0.3090 0.0126 11.00000 0.05 0.96 Q5 1 0.1538 0.2317 0.0849 11.00000 0.05 0.93 Q6 1 0.4236 1.0947 0.1379 11.00000 0.05 0.90 Q7 1 0.3239 0.4219 0.1922 11.00000 0.05 0.89 Q8 1 0.1227 0.3831 0.0505 11.00000 0.05 0.88 ; _shelx_res_checksum 58524 _shelx_hkl_file ; -1 0 -1 3.92 16.76 1 0 1 12.91 15.01 1 0 1 48.22 14.80 1 0 1 13.49 16.59 -1 0 -1 4.87 17.28 1 0 1 27.29 13.33 0 1 1 129.18 14.39 0 1 1 165.13 21.98 0 -1 1 135.76 20.25 0 1 -1 109.85 19.50 0 1 1 145.98 20.43 0 1 -1 117.61 24.70 0 -1 -1 123.52 12.67 0 -1 -1 122.56 20.63 0 -1 1 107.11 25.91 -1 -1 0 43.76 21.69 -1 1 0 -35.39 21.61 1 -1 0 3.57 26.52 -1 1 0 4.30 18.37 1 1 0 13.95 21.59 -1 1 0 3.56 42.55 1 1 0 16.32 3.03 1 -1 0 44.97 20.53 1 1 0 51.98 17.54 1 1 0 13.25 2.32 1 -1 0 34.33 18.24 -1 -1 0 1.31 27.84 -1 -1 2 3550.59 116.30 -1 1 2 3521.27 113.59 -1 1 2 3585.37 135.94 1 -1 -2 3355.81 100.29 -1 1 2 3594.42 134.63 1 -1 -2 3463.76 152.28 1 1 -2 3508.08 95.95 -1 -1 2 3596.05 175.51 1 1 -2 3455.34 129.48 1 0 -3 -0.96 4.64 1 0 -3 10.30 15.35 -1 0 3 5.19 5.41 -1 0 3 20.11 15.80 1 -1 2 1752.17 124.11 1 -1 2 2119.10 89.29 -1 1 -2 2000.22 97.23 1 1 2 1867.43 89.33 1 1 2 2010.44 50.10 -1 -1 -2 1898.01 90.63 -1 1 -2 1972.84 88.36 -1 1 -2 1796.25 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